• Title/Summary/Keyword: Spectrophotometry

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Solvent Effects on the Nucleophilc Addition (I) Effect of Solvent Polarity on the Nucleophilic Addition of Amine to Phenylvinylketone (친핵성 첨가반응에 대한 용매효과 (I) Phenylvinylketone에 대한 아민의 첨가반응속도에 미치는 용매의 극성효과)

  • Gap-Cheol Shin;Tae-Rin Kim
    • Journal of the Korean Chemical Society
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    • v.36 no.2
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    • pp.287-292
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    • 1992
  • The rate constants of the nucleophilic addition reaction of amines (piperidine and diethylamine) to phenylvinylketone in various solvents have been determined by UV spectrophotometry at $25^{\circ}C$. On the basis of the high sensitivity of the rate to the polarity of the medium, it may be concluded that the reaction intermediate has zwitterionic character. The effect of the solvents on the rate of the bimolecular nucleophilic addition reaction is described well by the Kirkwood equation: The transition state of the reaction has a cyclic structure formed through an intramolecular hydrogen bond. The addition reaction of primary and secondary amines to phenylvinylketone in all solvents take place considerably faster than that of tertiary amine and this results also can be explained by the intermediate products in the reaction have a cyclic structure formed through an intramolecular hydrogen bond for the primary and secondary amines but not for the tertiary amine.

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Formation and Dissociation Kinetics of Tetraaza-Crown-Alkanoic Acid Complexes of Cerium(Ⅲ)

  • 최기영;김동원;정용순;김창석;홍춘표;이용일
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.671-676
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    • 1998
  • The formation and dissociation rates of $Ce^{3+}$ Complexes of the 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-NN', N",N"'-tetraacetic acid (1), 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-N,N',N",N"'-tetramethylacetic acid (2), and 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-N,N',N",N"'-tetrapropionic acid (3) have been measured by the use of stopped-flow spectrophotometry. Observations were made at 25.0±0.1 ℃ and at an ionic strength of 0.10 M $NaClO_4$. The complexation of $Ce^{3+}$ ion with 1 and 2 proceeds through the formation of an intermediate complex $(CeH_3L^{2+})^*$ in which the $Ce^{3+}$ ion is incompletely coordinated. This may then lead to be a final product in the rate-determining step. Between pH 4.76 and 5.76, the diprotonated $(H_2L^{2-})$ from is revealed to be a kinetically active species despite of its low concentration. The stability constants $(logK(CeH_3L^{2+}))$ and specific water-assisted rate constants $(k_{OH})$ of intermediate complexes have been determined from the kinetic data. The dissociation reactions of $Ce^{3+}$ complexes of 1, 2, and 3 were investigated with $Cu^{2+}$, ions as a scavenger in acetate buffer. All complexes exhibit acid-independent and acid-catalyzed contributions. The effect of buffer and $Cu^{2+}$ concentration on the dissociation rate has also been investigated. The ligand effect on the dissociation rate of $Ce^{3+}$ complexes is discussed in terms of the side-pendant arms and the chelate ring sizes of the ligands.

Detection of Single Nucleotide Polymorphism in Human IL-4 Receptor by PCR Amplification of Specific Alleles

  • Hwang, Sue Yun;Kim, Seung Hoon;Hwang, Sung Hee;Cho, Chul Soo;Kim, Ho Youn
    • Animal cells and systems
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    • v.5 no.2
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    • pp.153-156
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    • 2001
  • A key aspect of genomic research in the “post-genome era”is to associate sequence variations with heritable phenotypes. The most common variations in the human genome are single nucleotide polymorphisms (SNPs) that occur approximately once in every 500 to 1,000 bases. Although analyzing the phenotypic outcome of these SNPs is crucial to facilitate large-scale association studies of genetic diseases, detection of SNPs from an extended number of human DNA samples is often difficult, labor-intensive and time-consuming. Recent development in SNP detection methods using DNA microarrays and mass spectrophotometry has allowed automated high throughput analyses, but such equipments are not accessible to many scientists. In this study, we demonstrate that a simple PCR-based method using primers with a mismatched base at the 3'-end provides a fast and easy tool to identify known SNPs from human genomic DNA in a regular molecular biology laboratory. Results from this PCR amplification of specific alleles (PASA) analysis efficiently and accurately typed the Q576R polymorphism of human IL4 receptor from the genomic DNAs of 29 Koreans, including 9 samples whose genotype could not be discerned by the conventiona1 PCR-SSCP (single strand conformation polymorphism) method. Given the increasing attention to disease-associated polymorphisms in genomic research, this alternative technique will be very useful to identify SNPs in large-scale population studies.

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Method development and validation of spectrophotometric and RP-HPLC methods for simultaneous estimation of spironolactone and furosemide in bulk and combined tablet dosage forms

  • Chavan, Rohankumar R.;Bhinge, Somnath D.;Bhutkar, Mangesh A.;Randive, Dheeraj S.;Salunkhe, Vijay R.
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.212-224
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    • 2021
  • The intent of the present work was to develop a simple, sensitive, accurate, precise, rapid and economical UV- spectrophotometric and reverse phase high pressure liquid chromatographic method for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms. UV-Spectrophotometry was carried out by simultaneous equation method using 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile (50:50) v/v as a solvent. The linearity range was 2-14 ㎍ mL-1 for Spironolactone and Furosemide with a correlation coefficient > 0.99. The chromatographic separation was achieved on 250 mm × 4.6 mm, hypersil BDS C18 column with particle size 5 ㎛, by using an isocratic mixture of 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile: tert butyl methyl ether (49:50:1) v/v/v as a solvent at a flow rate of 1 mL min-1 and UV detection was carried out at 254 nm. The retention time were observed to be 3.666 and 6.661 minutes for Furosemide and Spironolactone respectively. The two developed methods were validated according to the ICH guidelines for accuracy, precision, linearity, LOD, LOQ and were found to be within the limits. It can be concluded that these two methods could be successfully used for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms.

Antioxidant activities of brown teff hydrolysates produced by protease treatment

  • Yun, Ye-Rang;Park, Sung-Hee
    • Journal of Nutrition and Health
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    • v.51 no.6
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    • pp.599-606
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    • 2018
  • Purpose: Various plants, herbal medicines, and marine foodstuffs have been used in kimchi preparation to improve its overall quality. Teff, which is rich in minerals and starches, facilitates stable blood glucose levels and is well-suited for use in gluten-free products; hence, it can be used to reinforce the mineral composition of kimchi. In this study, we probed the antioxidant activities of hydrolysates prepared by treatment of brown teff with three proteases under different conditions. Methods: The mineral composition of brown teff was determined by inductively coupled plasma spectrophotometry-mass spectrometry, and we established optimal hydrolysis conditions by determining the total phenol and flavonoid contents of teff hydrolysates obtained using three different proteases (protamax, flavourzyme, and alcalase), two different protease concentrations (1 and 3 wt%), and three different incubation times (1, 2, and 4 h). The antioxidant activity of the hydrolysates was further investigated using 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging activity, total antioxidant capacity (TAC), and ferrous reducing antioxidant power (FRAP) assays. Results: Brown teff was rich in I, K, Mg, and Ca, and the highest total phenol content ($24.16{\mu}g/mL$), total flavonoid content ($69.08{\mu}g/mL$), and TAC were obtained for 1 wt% protamax treatment. However, the highest DPPH scavenging activity and FRAP values were observed for hydrolysates produced by alcalase and flavourzyme treatments, respectively. Conclusion: Treatment of brown teff with proteases affords hydrolysates with significantly increased antioxidant activities and high total phenol and flavonoid contents, and these antioxidant activities of teff hydrolysates have the potential to enhance the quality and functionality of kimchi in future applications.

Characteristics of Cu-Doped Ge8Sb2Te11 Thin Films for PRAM (PRAM용 Cu-도핑된 Ge8Sb2Te11 박막의 특성)

  • Kim, Yeong-Mi;Kong, Heon;Kim, Byung-Cheul;Lee, Hyun-Yong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.32 no.5
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    • pp.376-381
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    • 2019
  • In this work, we evaluated the structural, electrical and optical properties of $Ge_8Sb_2Te_{11}$ and Cu-doped $Ge_8Sb_2Te_{11}$ thin films prepared by rf-magnetron reactive sputtering. The 200-nm-thick deposited films were annealed in a range of $100{\sim}400^{\circ}C$ using a furnace in an $N_2$ atmosphere. The amorphous-to-crystalline phase changes of the thin films were investigated by X-ray diffraction (XRD), UV-Vis-IR spectrophotometry, a 4-point probe, and a source meter. A one-step phase transformation from amorphous to face-centered-cubic (fcc) and an increase of the crystallization temperature ($T_c$) was observed in the Cu-doped film, which indicates an enhanced thermal stability in the amorphous state. The difference in the optical energy band gap ($E_{op}$) between the amorphous and crystalline phases was relatively large, approximately 0.38~0.41 eV, which is beneficial for reducing the noise in the memory devices. The sheet resistance($R_s$) of the amorphous phase in the Cu-doped film was about 1.5 orders larger than that in undoped film. A large $R_s$ in the amorphous phase will reduce the programming current in the memory device. An increase of threshold voltage ($V_{th}$) was seen in the Cu-doped film, which implied a high thermal efficiency. This suggests that the Cu-doped $Ge_8Sb_2Te_{11}$ thin film is a good candidate for PRAM.

Influence of polishing systems on roughness and color change of two dental ceramics

  • Maciel, Lucas Campagnaro;Silva, Carlos Frederico Bettcher;de Jesus, Ricardo Huver;da Silva Concilio, Lais Regiane;Kano, Stefania Carvalho;Xible, Anuar Antonio
    • The Journal of Advanced Prosthodontics
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    • v.11 no.4
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    • pp.215-222
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    • 2019
  • PURPOSE. To evaluate the polishing effect on roughness and color change of pressed and layering ceramics after immersion in coffee solution. MATERIALS AND METHODS. 88 ceramic discs ($1.0mm{\times}10.0mm$) were manufactured - 44 nano-fluorapatite layering ceramics (IPS e.max Ceram. Group C) and 44 pressed lithium disilicate ceramic discs (IPS e. max Press - Group P). Each group was divided into 4 subgroups according to surface treatments: (G) Glaze, (S) Shofu polishing system (Shofu Inc.), (E) Edenta AG polishing System, (KG) $30-{\mu}m$ diamond granulation tip. Surface roughness (Ra) and color change (${\Delta}E$) measurings after the surface treatments were performed, before and 12 days after the immersion in coffee solution. A samples' qualitative analysis was conducted with a scanning electron microscopy (SEM). Data were statistically-treated with one-way-ANOVA and Duncan's tests, apart from paired t-test and Pearson's correlation test (${\alpha}=5%$). RESULTS. The decrescent order, both for surface roughness (Ra) and ${\Delta}E$ for both ceramics were: KG > E > S > G (P<.05). With exception for PG and CG subgroups, which did not present statistical difference between them, all other pressed ceramics subgroups presented smaller Ra values and greater ${\Delta}E$ values than the layering ceramics subgroups (P<.05). CONCLUSION. Although mechanical polishing systems presented intermediate Ra values, their colors were considered clinically acceptable. There is a strong correlation between the surface roughness and the color change of tested ceramics.

Choice of resin cement shades for a high-translucency zirconia product to mask dark, discolored or metal substrates

  • Dai, Shiqi;Chen, Chen;Tang, Mo;Chen, Ying;Yang, Lu;He, Feng;Chen, Bingzhuo;Xie, Haifeng
    • The Journal of Advanced Prosthodontics
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    • v.11 no.5
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    • pp.286-296
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    • 2019
  • PURPOSE. The aim was to study the masking ability of high-translucency monolithic zirconia and provide guidance in selecting resin luting cements in order to mask discolored substrates. MATERIALS AND METHODS. 160 high-translucency zirconia specimens were divided into 32 groups depending on their thickness and shades. Using five shades of try-in paste, the specimens were luted onto the substrates (Co-Cr, precious-metal, opaque porcelain-sintered Co-Cr, opaque porcelain-sintered precious-metal, and 5M3-shade zirconia). All CIELAB color parameters were measured and statistically analyzed. RESULTS. Zirconia shade and thickness and try-in paste shade affected CIELAB color parameters (P=.000) in different substrates groups, and there were interactions among these factors (P=.000). All five try-in paste shades can be chosen to achieve ${\Delta}E$ values of zirconia with 1.2 - 1.5 mm for masking dark-tooth-like 5M3-shade and zirconia with 1.5 mm for masking precious-metal groups < 2.6. Only suitable try-in paste shades were used, can ${\Delta}E$ values that less than 2.6 be achieved when applied translucent monolithic zirconia with 0.7-1.0 mm for masking dark-tooth-like 5M3-shade and zirconia with 0.7 - 1.2 mm for masking precious-metal groups. CONCLUSION. Choosing suitable resin cement shades is necessary for high-translucency monolithic zirconia to achieve ideal masking ability (${\Delta}E$ < 2.6) on the dark-tooth.

Development of Ultra-Thin TiO2 Coated WO3 Inverse Opal Photoelectrode for Dye-Sensitized Solar Cells (염료감응형 태양전지로의 응용을 위한 얇은 TiO2가 코팅 된 WO3 역오팔 광전극의 개발)

  • Arunachalam, Maheswari;Kwag, Seoui;Lee, Inho;Kim, Chung Soo;Lee, Sang-Kwon;Kang, Soon Hyung
    • Korean Journal of Materials Research
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    • v.29 no.8
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    • pp.491-496
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    • 2019
  • In this study, we prepare pure $WO_3$ inverse opal(IO) film with a thickness of approximately $3{\mu}m$ by electrodeposition, and an ultra-thin $TiO_2$ layer having a thickness of 2 nm is deposited on $WO_3$ IO film by atomic layer deposition. Both sets of photoelectrochemical properties are evaluated after developing dye-sensitized solar cells(DSSCs). In addition, morphological, crystalline and optical properties of the developed films are evaluated through field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HR-TEM), X-ray diffraction(XRD) and UV/visible/infrared spectrophotometry. In particular, pure $WO_3$ IO based DSSCs show low $V_{OC}$, $J_{SC}$ and fill factor of 0.25 V, $0.89mA/cm^2$ and 18.9 %, achieving an efficiency of 0.04 %, whereas the $TiO_2/WO_3$ IO based DSSCs exhibit $V_{OC}$, $J_{SC}$ and fill factor of 0.57 V, $1.18mA/cm^2$ and 50.1 %, revealing an overall conversion efficiency of 0.34 %, probably attributable to the high dye adsorption and suppressed charge recombination reaction.

Gold Nanoparticles Conjugation Enhances Antiacanthamoebic Properties of Nystatin, Fluconazole and Amphotericin B

  • Anwar, Ayaz;Siddiqui, Ruqaiyyah;Shah, Muhammad Raza;Khan, Naveed Ahmed
    • Journal of Microbiology and Biotechnology
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    • v.29 no.1
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    • pp.171-177
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    • 2019
  • Parasitic infections have remained a significant burden on human and animal health. In part, this is due to lack of clinically-approved, novel antimicrobials and a lack of interest by the pharmaceutical industry. An alternative approach is to modify existing clinically-approved drugs for efficient delivery formulations to ensure minimum inhibitory concentration is achieved at the target site. Nanotechnology offers the potential to enhance the therapeutic efficacy of drugs through modification of nanoparticles with ligands. Amphotericin B, nystatin, and fluconazole are clinically available drugs in the treatment of amoebal and fungal infections. These drugs were conjugated with gold nanoparticles. To characterize these gold-conjugated drug, atomic force microscopy, ultraviolet-visible spectrophotometry and Fourier transform infrared spectroscopy were performed. These drugs and their gold nanoconjugates were examined for antimicrobial activity against the protist pathogen, Acanthamoeba castellanii of the T4 genotype. Moreover, host cell cytotoxicity assays were accomplished. Cytotoxicity of these drugs and drug-conjugated gold nanoparticles was also determined by lactate dehydrogenase assay. Gold nanoparticles conjugation resulted in enhanced bioactivity of all three drugs with amphotericin B producing the most significant effects against Acanthamoeba castellanii (p < 0.05). In contrast, bare gold nanoparticles did not exhibit antimicrobial potency. Furthermore, amoebae treated with drugs-conjugated gold nanoparticles showed reduced cytotoxicity against HeLa cells. In this report, we demonstrated the use of nanotechnology to modify existing clinically-approved drugs and enhance their efficacy against pathogenic amoebae. Given the lack of development of novel drugs, this is a viable approach in the treatment of neglected diseases.